CN114734049A - Method for preparing ultra-small nano silver by using sodium borohydride - Google Patents
Method for preparing ultra-small nano silver by using sodium borohydride Download PDFInfo
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- CN114734049A CN114734049A CN202210248383.9A CN202210248383A CN114734049A CN 114734049 A CN114734049 A CN 114734049A CN 202210248383 A CN202210248383 A CN 202210248383A CN 114734049 A CN114734049 A CN 114734049A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000012279 sodium borohydride Substances 0.000 title claims abstract description 55
- 229910000033 sodium borohydride Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 39
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 108
- 238000003756 stirring Methods 0.000 claims abstract description 66
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 238000005303 weighing Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000004321 preservation Methods 0.000 claims description 15
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 132
- 239000000843 powder Substances 0.000 description 32
- 239000002245 particle Substances 0.000 description 28
- 239000007787 solid Substances 0.000 description 18
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 12
- 238000009826 distribution Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 241000606153 Chlamydia trachomatis Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000588653 Neisseria Species 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- -1 alkyl sulfur Chemical compound 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229940038705 chlamydia trachomatis Drugs 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a method for preparing ultra-small nano silver by using sodium borohydride, which relates to the technical field of nano metal material preparation and comprises the following steps: weighing a certain amount of silver nitrate, PVP and sodium borohydride, and respectively dissolving the weighed silver nitrate and PVP in deionized water to prepare a silver nitrate solution and a PVP solution; slowly dripping a PVP solution into a silver nitrate solution for mixing, simultaneously fully stirring to obtain solution A, then dissolving weighed sodium borohydride into deionized water, and fully stirring to obtain solution B; and finally, slowly dripping the solution B into the solution A through a separating funnel, and after the solution A is uniformly stirred and maintained, completing the preparation of the nano silver. The invention has the beneficial effects that: the method has the advantages of easily available raw materials, simple operation of the preparation process, mild reaction conditions, strong practicability and good reproducibility, is suitable for industrial mass production, and is beneficial to practical application.
Description
Technical Field
The invention relates to the technical field of nano metal material preparation, in particular to a method for preparing ultra-small nano silver by using sodium borohydride.
Background
The nano silver is a metal silver simple substance with the particle size of nano grade, the particle size of the nano silver is mostly about 25 nm, the nano silver has strong inhibiting and killing effects on dozens of pathogenic microorganisms such as escherichia coli, gonococcus, chlamydia trachomatis and the like, and drug resistance can not be generated, the nano silver material has stable physical and chemical properties such as high thermal conductivity, high electrical conductivity, excellent optical properties and the like, and can be widely applied to the aspects of electricity, optics, catalysis, biosensors, data storage, magnetic devices, medical antibiosis, surface enhanced Raman spectroscopy and the like, the nano silver with different shapes has different properties, such as small particle size, and spherical nano silver with narrow particle size distribution has good antibacterial property and conductive property.
The preparation method of the nano silver has various methods, and China mainly adopts a physical method and a chemical reduction method, wherein the physical method can obtain the nano silver powder with higher purity, but the method has the defects of high production cost, large investment, low yield, high industrialization difficulty and the like, and is not suitable for the current economic conditions and industrial foundations. The chemical reduction method generally adopts silver nitrate aqueous solution or silver ammonia solution, adds proper surfactant as nano silver surface protective agent, the surfactant generally adopts alkyl sulfur, oleic acid or palmitic acid, then adds proper reducing agent, reduces the silver in the silver nitrate solution or silver ammonia solution into nano silver particles, centrifugalizes to obtain precipitate, repeatedly washes the precipitate with deionized water, dries in vacuum to obtain nano silver powder, and the nano silver prepared by the method has the problems of low yield, complex process, difficult control, certain difficulty in industrial production, expensive raw material, large particle size of the prepared nano silver, and is not beneficial to practical application, so the development of a preparation method of the ultra-small-size nano silver is urgently needed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing ultra-small nano silver by using sodium borohydride, which solves the problems in the background technology.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for preparing ultra-small nano silver by using sodium borohydride comprises the following steps:
s1, weighing a certain amount of silver nitrate, PVP and sodium borohydride, and respectively dissolving the weighed silver nitrate and PVP in deionized water to prepare a silver nitrate solution and a PVP solution;
s2, slowly dripping the PVP solution into the silver nitrate solution for mixing, simultaneously fully stirring to obtain solution A, then dissolving the weighed sodium borohydride into deionized water, and fully stirring to obtain solution B;
and S3, respectively heating the solution A and the solution B in a water bath, slowly dripping the solution B into the solution A through a separating funnel after the temperature is constant, and placing the solution B into a magnetic stirrer for continuous heat preservation and stirring after the dripping of the solution B is finished, thus completing the preparation of the nano silver.
Optionally, the concentration of the silver nitrate solution in the step S1 is 1 mmol/L.
Optionally, the concentration of the PVP solution in the step S1 is 0.3%.
Optionally, the concentration of the solution B prepared in the step S2 is 0.5 to 30mmol/L, and the reaction temperature in the preparation process is 25 ℃.
Optionally, the time for two times of sufficient stirring in step S2 is 30 min.
Optionally, the time for continuing the heat preservation stirring in step S3 is 120 min.
Optionally, in the step S3, the stirring speed of the magnetic stirrer continuing to perform heat preservation stirring is 800 r/min.
Optionally, the average particle size of the nano silver prepared in step S3 is 3-30 nm.
The invention provides a method for preparing ultra-small nano silver by using sodium borohydride, which has the following beneficial effects:
1. the invention has the advantages of simple adopted equipment, easily obtained raw materials, low cost and convenient large-scale popularization and use.
2. The whole process for preparing the nano-silver has mild reaction conditions and good reproducibility.
3. The average grain size of the nano silver prepared by the method is 3-30nm, and the grain size is far smaller than that of the nano silver prepared by other complex processes and methods.
Drawings
FIG. 1 is a diagram of the UV-Vis spectrum of the nano-silver prepared in the first example;
FIG. 2 is a diagram of the UV-Vis spectrum of the nano-silver prepared in example two;
FIG. 3 is a UV-Vis spectrum of the nano-silver prepared in the third example;
FIG. 4 is a UV-Vis spectrum of nano-silver prepared in example four;
FIG. 5 is a UV-Vis spectrum of nano-silver prepared in example V;
FIG. 6 is a UV-Vis spectrum of nano-silver prepared in example six;
fig. 7 is a statistical chart of the average particle size of the nano silver prepared in the first to sixth examples.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1 to 7, the present invention provides a technical solution: a method for preparing ultra-small nano silver by using sodium borohydride comprises the following steps:
s1, weighing a certain amount of silver nitrate, PVP and sodium borohydride, and respectively dissolving the weighed silver nitrate and PVP in deionized water to prepare a silver nitrate solution and a PVP solution;
s2, slowly dripping the PVP solution into the silver nitrate solution for mixing, simultaneously fully stirring to obtain solution A, then dissolving the weighed sodium borohydride into deionized water, and fully stirring to obtain solution B;
and S3, respectively heating the solution A and the solution B in a water bath, slowly dripping the solution B into the solution A through a separating funnel after the temperature is constant, and placing the solution B into a magnetic stirrer to continuously stir at a constant temperature after the dripping of the solution B is finished, so that the preparation of the nano silver is finished.
The concentration of the silver nitrate solution in the step S1 is 1mmol/L, so that the prepared silver nitrate solution is better limited in concentration, and subsequent preparation operation is facilitated.
The concentration of the PVP solution in the step S1 is 0.3%, so that the concentration of the PVP solution is better limited, and the PVP solution and a silver nitrate solution are conveniently matched for use, and a preparation effect is achieved.
Wherein the concentration of the solution B prepared in the step S2 is 0.5-30mmol/L, the reaction temperature in the preparation process is 25 ℃, and the simple preparation condition is beneficial to industrial mass production.
Wherein, the time of the two times of full stirring in the step S2 is 30min, and the full stirring time is set, so that the stirring and mixing effects can be better ensured.
In step S3, the time for continuing the heat preservation stirring is 120min, and the heat preservation stirring time is set to better ensure that the liquid a and the liquid B can be fully mixed and reacted.
In the step S3, the stirring speed of the magnetic stirrer continuing to perform heat preservation stirring is 800r/min, when the stirring speed is too slow, PVP molecules are not enough to completely wrap the nano silver and the reaction is incomplete, and when the stirring speed is too fast, the stability of the nano silver colloidal solution is destroyed, so that the stirring speed of 800r/min needs to be selected for heat preservation stirring, thereby ensuring the preparation effect.
Wherein the average particle size of the nano silver prepared in the step S3 is 3-30 nm.
The beneficial effects of the present invention are illustrated by the following specific examples:
the first embodiment of the invention provides a method for preparing ultra-small nano silver by using sodium borohydride, which comprises the following steps:
step one, weighing 17mg of silver nitrate solid, adding the silver nitrate solid into 100.0ml of deionized water, heating and stirring to dissolve the silver nitrate solid to form a transparent and uniform silver nitrate solution, meanwhile, weighing 0.3g of PVP powder, adding the PVP powder into 100.0ml of deionized water, heating and stirring to fully dissolve the PVP powder to form a transparent and uniform PVP solution;
step two, slowly dripping the PVP solution obtained in the step one into a silver nitrate solution, stirring the solution for 1 hour to fully mix the solution to obtain solution A, then weighing 3.8mg of sodium borohydride powder, adding the sodium borohydride powder into 100.0ml of deionized water, heating and stirring the solution to fully dissolve the sodium borohydride to form a transparent and uniform sodium borohydride solution with the concentration of 1mmol/L, and obtaining solution B;
and step three, heating the solution A and the solution B obtained in the step two to room temperature through water bath, slowly dripping the solution B into the solution A through a separating funnel within 15min after the temperature is constant, placing the solution B into a magnetic stirrer after the dripping of the solution B is finished, setting the stirring speed to be 800r/min, and continuing to stir for 120min under the condition of heat preservation, thus finishing the preparation of the nano silver.
FIG. 1 is the UV-Vis spectrum of the nano-silver obtained in the first example. And a nano-particle size analyzer is adopted to characterize the particle size distribution state of the nano-silver particles in the product, and the average size of the obtained nano-silver particles is 23 nm.
The second embodiment of the invention provides a method for preparing ultra-small nano silver by using sodium borohydride, which comprises the following steps:
step one, weighing 17mg of silver nitrate solid, adding the silver nitrate solid into deionized water, heating and stirring to dissolve the silver nitrate solid to form a transparent and uniform silver nitrate solution with the concentration of 1mmol/L, meanwhile, weighing 0.3g of PVP powder, adding the PVP powder into 100.0ml of deionized water, heating and stirring to fully dissolve the PVP powder to form a transparent and uniform PVP solution;
step two, slowly dropwise adding the PVP solution obtained in the step one into a silver nitrate solution, stirring the solution for 1 hour to fully mix the solution to obtain solution A, then weighing 7.6mg of sodium borohydride powder, adding the sodium borohydride powder into deionized water, heating and stirring the deionized water to fully dissolve the sodium borohydride to form a transparent and uniform sodium borohydride solution with the concentration of 2mmol/L, and obtaining solution B;
and step three, heating the solution A and the solution B obtained in the step two to room temperature through water bath, slowly dripping the solution B into the solution A through a separating funnel within 30min after the temperature is constant, placing the solution B into a magnetic stirrer after the dripping of the solution B is finished, setting the stirring speed to be 800r/min, and continuing to stir for 120min under heat preservation, thus finishing the preparation of the nano silver.
FIG. 2 is the UV-Vis spectrum of the nano-silver obtained in example two. And a nano-particle size analyzer is adopted to characterize the particle size distribution state of the nano-silver particles in the product, and the average size of the obtained nano-silver particles is 15 nm.
The third embodiment of the invention provides a method for preparing ultra-small nano silver by using sodium borohydride, which comprises the following steps:
weighing 17mg of silver nitrate solid, adding the silver nitrate solid into deionized water, heating and stirring to dissolve the silver nitrate solid to form a transparent and uniform silver nitrate solution with the concentration of 1mmol/L, meanwhile, weighing 0.3g of PVP powder, adding the PVP powder into 100.0ml of deionized water, heating and stirring to fully dissolve the PVP powder to form a transparent and uniform PVP solution;
step two, slowly dropwise adding the PVP solution obtained in the step one into a silver nitrate solution, stirring the solution for 1 hour to fully mix the solution to obtain solution A, then weighing 38.0mg of sodium borohydride powder, adding the sodium borohydride powder into deionized water, heating and stirring the deionized water to fully dissolve the sodium borohydride to form a transparent and uniform sodium borohydride solution with the concentration of 10mmol/L, and obtaining solution B;
and step three, heating the solution A and the solution B obtained in the step two to room temperature through water bath, slowly dripping the solution B into the solution A through a separating funnel within 18min after the temperature is constant, placing the solution B into a magnetic stirrer after the dripping of the solution B is finished, setting the stirring speed to be 800r/min, and continuing to stir for 120min under heat preservation, thus finishing the preparation of the nano silver.
FIG. 3 is the UV-Vis spectrum of the nano-silver obtained in example III. And a nano-particle size analyzer is adopted to characterize the particle size distribution state of the nano-silver particles in the product, and the average size of the obtained nano-silver particles is 10 nm.
The fourth embodiment of the present invention provides a method for preparing ultra-small nano silver by using sodium borohydride, comprising the following steps:
weighing 17mg of silver nitrate solid, adding the silver nitrate solid into deionized water, heating and stirring to dissolve the silver nitrate solid to form a transparent and uniform silver nitrate solution with the concentration of 1mmol/L, meanwhile, weighing 0.3g of PVP powder, adding the PVP powder into 100.0ml of deionized water, heating and stirring to fully dissolve the PVP powder to form a transparent and uniform PVP solution;
step two, slowly dropwise adding the PVP solution obtained in the step one into a silver nitrate solution, stirring the solution for 1 hour to fully mix the solution to obtain solution A, then weighing 76mg of sodium borohydride powder, adding the sodium borohydride powder into deionized water, heating and stirring the deionized water to fully dissolve the sodium borohydride to form a transparent and uniform sodium borohydride solution with the concentration of 20mmol/L, and obtaining solution B;
and step three, heating the solution A and the solution B obtained in the step two to room temperature through water bath, slowly dripping the solution B into the solution A through a separating funnel within 20min after the temperature is constant, placing the solution B into a magnetic stirrer after the dripping of the solution B is finished, setting the stirring speed to be 800r/min, and continuing to stir for 120min under heat preservation, thus finishing the preparation of the nano silver.
FIG. 4 is the UV-Vis spectrum of the nano-silver obtained in example four. And a nano particle size analyzer is adopted to characterize the particle size distribution state of the nano silver particles in the product, and the average size of the obtained nano silver particles is 3 nm.
The fifth embodiment of the present invention provides a method for preparing ultra-small silver nanoparticles using sodium borohydride, comprising the following steps:
weighing 17mg of silver nitrate solid, adding the silver nitrate solid into deionized water, heating and stirring to dissolve the silver nitrate solid to form a transparent and uniform silver nitrate solution with the concentration of 1mmol/L, meanwhile, weighing 0.3g of PVP powder, adding the PVP powder into 100.0ml of deionized water, heating and stirring to fully dissolve the PVP powder to form a transparent and uniform PVP solution;
step two, slowly dropwise adding the PVP solution obtained in the step one into a silver nitrate solution, stirring the solution for 1 hour to fully mix the solution to obtain solution A, then weighing 95mg of sodium borohydride powder, adding the sodium borohydride powder into deionized water, heating and stirring the deionized water to fully dissolve the sodium borohydride to form a transparent and uniform sodium borohydride solution with the concentration of 25mmol/L, and obtaining solution B;
and step three, heating the solution A and the solution B obtained in the step two to room temperature through water bath, slowly dripping the solution B into the solution A through a separating funnel within 20min after the temperature is constant, placing the solution B into a magnetic stirrer after the dripping of the solution B is finished, setting the stirring speed to be 800r/min, and continuing to stir for 120min under heat preservation, thus finishing the preparation of the nano silver.
FIG. 5 is the UV-Vis spectrum of the nano-silver obtained in example V. And a nano-particle size analyzer is adopted to characterize the particle size distribution state of the nano-silver particles in the product, and the average size of the obtained nano-silver particles is 5 nm.
The sixth embodiment of the present invention provides a method for preparing ultra-small nano silver by using sodium borohydride, comprising the following steps:
weighing silver nitrate solid, adding the silver nitrate solid into deionized water, heating and stirring to dissolve the silver nitrate solid to form a transparent and uniform silver nitrate solution with the concentration of 1mmol/L, meanwhile, weighing 0.3g of PVP powder, adding the PVP powder into 100.0ml of deionized water, heating and stirring to fully dissolve the PVP powder to form a transparent and uniform PVP solution;
step two, slowly dripping the PVP solution obtained in the step one into a silver nitrate solution, stirring the solution for 1 hour to fully mix the solution to obtain solution A, then weighing 114mg of sodium borohydride powder, adding the sodium borohydride powder into deionized water, heating and stirring the deionized water to fully dissolve the sodium borohydride to form a transparent and uniform sodium borohydride solution with the concentration of 30mmol/L to obtain solution B;
and step three, heating the solution A and the solution B obtained in the step two to room temperature through water bath, slowly dripping the solution B into the solution A through a separating funnel within 25min after the temperature is constant, placing the solution B into a magnetic stirrer after the dripping of the solution B is finished, setting the stirring speed to be 800r/min, and continuing to stir for 120min under heat preservation, thus finishing the preparation of the nano silver.
FIG. 6 is a UV-Vis spectrum of the nano-silver obtained in example VI. And a nano-particle size analyzer is adopted to characterize the particle size distribution state of the nano-silver particles in the product, and the average size of the obtained nano-silver particles is 8 nm.
The concentrations of the silver nitrate solution, PVP solution, and sodium borohydride solution in examples one through six are shown in the following tables:
in summary, the average size of the nano silver particles prepared in the first to sixth examples is between 3nm and 30nm, as shown in fig. 7.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for preparing ultra-small nano silver by using sodium borohydride is characterized in that: the method comprises the following steps:
s1, weighing a certain amount of silver nitrate, PVP and sodium borohydride, and respectively dissolving the weighed silver nitrate and PVP in deionized water to prepare a silver nitrate solution and a PVP solution;
s2, slowly dripping the PVP solution into the silver nitrate solution for mixing, simultaneously fully stirring to obtain solution A, then dissolving the weighed sodium borohydride into deionized water, and fully stirring to obtain solution B;
and S3, respectively heating the solution A and the solution B in a water bath, slowly dripping the solution B into the solution A through a separating funnel after the temperature is constant, and placing the solution B into a magnetic stirrer to continuously stir at a constant temperature after the dripping of the solution B is finished, so that the preparation of the nano silver is finished.
2. The method for preparing ultra-small-size nano silver by using sodium borohydride according to claim 1, wherein the method comprises the following steps: the concentration of the silver nitrate solution in the step S1 is 1 mmol/L.
3. The method for preparing ultra-small-size nano silver by using sodium borohydride according to claim 1, wherein the method comprises the following steps: the concentration of the PVP solution in the step S1 was 0.3%.
4. The method for preparing ultra-small-size nano silver by using sodium borohydride according to claim 1, wherein the method comprises the following steps: the concentration of the solution B prepared in the step S2 is 0.5-30mmol/L, and the reaction temperature in the preparation process is 25 ℃.
5. The method for preparing ultra-small-size nano silver by using sodium borohydride according to claim 1, wherein the method comprises the following steps: the time for two times of full stirring in the step S2 is 30 min.
6. The method for preparing ultra-small-size nano silver by using sodium borohydride according to claim 1, which is characterized in that: the time for continuing the heat preservation stirring in the step S3 is 120 min.
7. The method for preparing ultra-small-size nano silver by using sodium borohydride according to claim 1, wherein the method comprises the following steps: and in the step S3, the stirring speed of the magnetic stirrer for continuously carrying out heat preservation stirring is 800 r/min.
8. The method for preparing ultra-small-size nano silver by using sodium borohydride according to claim 1, wherein the method comprises the following steps: the average grain diameter of the nano silver prepared in the step S3 is 3-30 nm.
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| CN202210248383.9A CN114734049A (en) | 2022-03-14 | 2022-03-14 | Method for preparing ultra-small nano silver by using sodium borohydride |
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